EP0685571B1 - Verfahren und Vorrichtung zur Beschichtung eines Substrats mittels Kathodenzerstäubung - Google Patents

Verfahren und Vorrichtung zur Beschichtung eines Substrats mittels Kathodenzerstäubung Download PDF

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Publication number
EP0685571B1
EP0685571B1 EP95870065A EP95870065A EP0685571B1 EP 0685571 B1 EP0685571 B1 EP 0685571B1 EP 95870065 A EP95870065 A EP 95870065A EP 95870065 A EP95870065 A EP 95870065A EP 0685571 B1 EP0685571 B1 EP 0685571B1
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EP
European Patent Office
Prior art keywords
target
surface layer
substrate
metal
elements
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP95870065A
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English (en)
French (fr)
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EP0685571A1 (de
Inventor
Pierre Vanden Brande (U.L.B.)
Stéphane Lucas (U.L.B.)
René Winand (U.L.B.)
Alain Weymeersch (Rd-Cs)
Lucien Renard (Rd-Cs)
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ArcelorMittal Liege Upstream SA
Original Assignee
Cockerill Sambre SA
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy

Definitions

  • the present invention relates to a method for formation of a coating on a substrate by sputtering ("sputtering") in an enclosure in the presence of an ionized gas, such as defined in the preamble of claim 1.
  • sputtering sputtering
  • an ionized gas such as defined in the preamble of claim 1.
  • the electrolysis technique involves the use of organic and inorganic chemical reagents whose effluents must be subjected to a neutralization treatment before rejection.
  • One of the essential aims of the present invention is to remedy these significant disadvantages of known methods and especially to allow to form light and compact non-porous deposits and very adherent of a certain thickness with an industrial yield valid. able. Moreover. be carried out without excessive heating of the support to be covered, thus allowing all the properties to be preserved initials of the latter.
  • the transfer is controlled thermal towards the surface layer of the target by regulating the cooling of this layer by means of a liquid substance conductive inserted between a cooling system and the layer surface of the target.
  • the invention also relates to a device for setting implementing the aforementioned process as defined in the preamble to the claim 9.
  • This process is characterized by the fact that means are provided including a thermal regulation system by means of a thermally conductive liquid substance interposed between a system of cooling and the surface layer of the target a system of heating which can optionally be incorporated between the layer surface and thermal transfer regulation system.
  • the invention also relates to a device for the implementation of the above method.
  • This process is characterized by the fact that means are provided to supply the layer surface of the target by the elements to be deposited on the substrate and to maintain or carry this layer superficial in the liquid state, so as to allow a distribution of the elements supplied on the surface of target.
  • the substrate is in the form of a continuous band moving through at least one enclosure in which a target is arranged and in which takes place sputtering from this target.
  • Figure 1 is a schematic view in elevation of part of this embodiment particular of the device according to the invention.
  • Figure 2 is, on a larger scale, a fully schematic view of a detail of this shape of achievement.
  • Figure 3 is a schematic view of this particular embodiment.
  • the invention relates first of all to a method for the formation of a coating on a substrate by sputtering in a enclosure maintained at a relatively low pressure, in presence of an ionized gas, according to which use is made a target with an oriented surface layer to the substrate containing at least one of the elements of the coating.
  • the surface layer of the target is formed by at least one of the elements following: Al, In, Bi, Li, Sn, Ga, Pb, Tl, Na, K, Rb and Fr and / or by at least one alloy of the above-mentioned metals.
  • Tin is particularly interesting because its vapor pressure is less than 10 -11 Torr at 530 ° C. As a result of this low vapor pressure, any problem of contamination of the walls of the enclosure by this metal is avoided below this temperature, even when a very high vacuum prevails in this enclosure.
  • Layer metal supply surface of the target takes place by adding a metal input either in the molten state or in a solid form as it melts on contact with this surface layer maintained above the melting temperature of metal but below the boiling point of the latter in working conditions.
  • the thickness of the surface layer at the target is preferably kept between 0.01 and 0.5 cm.
  • This device is characterized by particularly by the fact that it includes means to carry and maintain the above-mentioned surface layer of the target in the liquid state and regulate its temperature.
  • target 1 of this device includes a retention tank 2, the bottom 3 of which is formed from a block of material thermally conductive, such as copper or another metal having good thermoconductive properties, in which are incorporated a heating system 4, by example by electrical resistance, and a system of cooling 5, for example by water, between which there is a thermal transfer regulation system 6 comprising a circuit for a thermally conductive fluid.
  • a heating system 4 by example by electrical resistance
  • a system of cooling 5 for example by water
  • thermal transfer regulation system 6 comprising a circuit for a thermally conductive fluid.
  • the system of heating 4 is not essential for proper operation given that most of the heat required to melt the surface layer will come from plasma.
  • the magnets 7 of a magnetron conventional generally used in a cathode sputtering.
  • the retention tank 2 is intended for maintain a relatively thin surface layer 8 spray metal in the liquid state. Thickness of this layer is generally kept between 0.01 and 0.5 cm and is preferably of the order of 1 mm.
  • the heating system 4 is as close as possible to this surface layer, so as to allow a heat transfer as efficient as possible to the latter.
  • the regulation system 6 interposed, between the heating system 4 and the cooling system 5, includes a slot in which can be introduces the thermally conductive fluid.
  • the latter is preferably consisting of a liquid metal, especially gallium.
  • Figure 2 illustrates more concretely this regulation of the heat transfer between the metal liquid 8 contained in the retention tank 2 and the cooling system 5.
  • Tm indicates the temperature of the surface layer 8 or from the bottom of the retention tank 2
  • e1 indicates the thickness of the layer of the block of conductive material containing the heating system 4, if any.
  • This layer of conductive material is then followed by a space of thickness H, forming the above-mentioned slot, in which can be introduced the thermally conductive fluid.
  • h indicates the thickness of the fluid layer thermally conductive.
  • a new layer of the block of solid thermally conductive material of thickness e2 separates the thermally conductive fluid from the cooling 5, of which Te represents the temperature.
  • the level of liquid metal 8 in the tank retention 2 is controlled in this embodiment particular of the invention by means of two probes S1 and S2 operating by comparison of the measured voltage with the target's voltage.
  • the target 1 When the low level is reached, the target 1 is supplied with spray metal 13, while when the high level is reached, this feeding is stopped.
  • the probe S1 measures the maximum level, while the S2 probe measures the minimum level of the liquid metal layer 8.
  • the metal constituting the surface layer 8 is worn or maintained above its melting temperature and the this temperature is controlled by means of a S3 probe.
  • a backup heater can optionally be provided near supply area 9 to reach the melting temperature as well as for compensate for the latent heat of fusion of the metal.
  • the surface layer 8 can be in the solid state during spraying and is only melted to allow it to be fed or to help remove inequalities thickness of this layer caused by spraying in the solid state.
  • the feeding area is advantageously shielded by a metallic sheath 10 sufficiently close around the spray metal 13 introduced into the layer of liquid metal 8, to avoid the formation of a plasma.
  • a similar sheath 11 is also advantageously provided all around the edge of the retention tank 2.
  • a mechanism particular power supply 12 is provided for feeding the target surface layer 8 1 by spray metal 13 when the level of this layer descends below a determined limit, that is to say reaches the S2 probe.
  • This mechanism includes a reel, not shown in the figures, of a metal wire of spray 13 guided in a shielding tube 10, towards the liquid metal surface layer 8 of the target 1 to be melted as it enters in this layer.
  • the feed mechanism 12 is isolated electrically with respect to ground since it is at potential of target 1.
  • FIG. 3 schematically shows an embodiment of the cathode sputtering device according to the invention which may be suitable for the continuous coating or the passing of a strip on its two faces.
  • This device comprises two successive sputtering chambers 15 and 16 in which there is preferably a pressure between 10 -3 and 5.10 -2 Torr during the spraying.
  • each of these enclosures 15 and 16 is arranged a target 1 of the type shown in the figure 1, that is to say comprising a retention tank 2 containing spray metal 8 in the liquid state.
  • the substrate on which a coating must being deposited by sputtering is formed by an endless band 17, such as a sheet, moving successively through enclosure 15 and enclosure 16, against the respective targets 1.
  • the sheet 17 to be coated on its two sides is unwound from a reel 18 for cross the enclosure 15, where one of its faces is coated by spray metal. Then she goes into enclosure 16, after being guided on drums of reference 19 and 20, allowing to reverse its direction of displacement as it enters this enclosure 16 where the covering of the other side takes place by spray metal. Finally, at the exit of this enclosure 16 the strip covered on its two faces by spray metal is wound in a reel 21 for storage.
  • the following method and device the invention are particularly suitable for formation of tin and aluminum coatings on steel sheets.
  • the process currently used is based on the technique of electrolysis in aqueous solution, while the aluminum cladding is generally obtained by quenching of the steel sheet in a bath of molten metal.
  • the disadvantages of these two techniques have already been briefly described above.
  • the running speed of a metal strip to be covered will advantageously be between 300 and 600 m / min. for a deposition rate of 1 to 50 ⁇ m / min. and a target power density of 15 to 750 W / cm 2 .
  • the thermal production system uses gallium as a thermally conductive fluid.
  • the invention is not not limited to the concrete embodiment of the cathode sputtering process and device described above and shown in the appended figures, but that many variants can be envisaged without depart from the scope of the present invention.
  • the layer surface of the target can be maintained constantly in liquid state for the duration of the spraying, or, on the other hand, can only be worn in a molten state during and / or possibly some time after the filler metal supply towards this layer and / or again when areas erosion of a certain depth have formed in the solid surface layer next to the magnets of the magnetron.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Claims (17)

  1. Verfahren zum Beschichten eines Substrates (17) mittels Kathodenzerstäubung in einer Kammer (15, 16) in Gegenwart eines ionisierten Gases,
    wobei ein Target (1) verwendet wird, welches eine Oberflächenschicht (8) aufweist, die zum Substrat (17) hin orientiert ist und die mindestens eines der Elemente enthält, die auf dem Substrat (17) mittels Kathodenzerstäubung abgeschieden werden sollen,
    welches unter solchen Bedingungen durchgeführt wird, daß das oder die Elemente unter dem Einfluß des ionisierten Gases aus der Oberflächenschicht herausgeschleudert werden können, um sich anschließend auf dem Substrat (17) niederzuschlagen,
    und wobei während des Verfahrens der Oberflächenschicht des Targets die auf dem Substrat abzuscheidenden Elemente zugeführt werden und
    wobei diese Oberflächenschicht im flüssigen Zustand gehalten oder dahin überführt wird, um derart eine vorzugsweise merklich gleichmäßige Verteilung der Elemente, die der Oberfläche des Targets (1) zugeführt werden, zu erreichen,
    dadurch gekennzeichnet, daß
    der Wärmetransfer zur Oberflächenschicht (8) des Targets (1) durch eine Regelung zur Kühlung dieser Schicht mittels eines Kreislaufes für ein wärmeleitfähiges Fluid (6) kontrolliert wird,
    welcher zwischen einem Kühlsystem (5) und der Oberflächenschicht (8) des Targets (1) angeordnet ist.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß eine Oberflächenschicht (8) verwendet wird, die aus mindestens einem Metall gebildet ist, welches einen niedrigeren Dampfdruck als der in der Kammer (15, 16) herrschende Druck aufweist.
  3. Verfahren nach einem der Ansprüche 1 und 2, dadurch gekennzeichnet, daß eine Oberflächenschicht (8) verwendet wird, die aus mindestens einem Metall gebildet ist, welches einen Dampfdruck von weniger als 10-3 Torr und vorzugsweise weniger als 10-5 Torr aufweist.
  4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Oberflächenschicht (8) des Targets (1) aus mindestens einem der folgenden Elemente besteht: Al, In, Bi, Li, Sn, Ga, Pb, Tl, Na, K, Rb und Fr und/oder aus mindestens einer Legierung der genannten Metalle.
  5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Dicke der Oberflächenschicht (8) des Targets (1) derart aufrechterhalten wird, daß dieser zusätzliches Metall zugeführt wird, welches sich im schmelzflüssigen Zustand befindet oder welches bei Kontakt mit der Oberflächenschicht (8) des Targets (1) schmelzen kann.
  6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Dicke der flüssigen Oberflächenschicht (8) des Targets (1) zwischen 0,01 und 0,5 cm gehalten wird.
  7. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß das Substrat (17) merklich stetig in Bezug auf die Oberflächenschicht (8) des Targets (1) verschoben wird.
  8. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß in der Kammer (15, 16) ein Druck zwischen 0,133 Pa und 0,667 Pa (10-3 und 5 x 10-2 Torr) während der Zerstäubung aufrechterhalten wird.
  9. Vorrichtung zur Beschichtung eines Substrates (17) mittels Kathodenzerstäubung, umfassend mindestens eine Kammer (15, 16), in welcher sich das Substrat (17) und ein Target (1) befinden, welches eine Oberflächenschicht (8) aufweist, die zum letzteren hin orientiert ist und die mindestens eines der Beschichtungselemente enthält,
    dadurch gekennzeichnet, daß
    Mittel (4, 5, 6) vorgesehen sind, um der Oberflächenschicht (8) des Targets (1) die auf das Substrat (17) abzuscheidenden Elemente zuzuführen und um diese Oberflächenschicht (8) in flüssigem Zustand zu erhalten oder zu überführen,
    derart, daß eine Verteilung der zugeführten Elemente auf der Oberfläche des Targets (1) ermöglicht wird,
    dadurch gekennzeichnet, daß die Mittel ein System zur Wärmeregelung (6) umfassen, welches aus
    einem Kreislauf für ein wärmeleitfähiges Fluid besteht, der zwischen einem Kühlsystem (5) und der Oberflächenschicht (8) des Targets (1) angeordnet ist,
    und einem Heizsystem (4), das eventuell zwischen der Oberflächenschicht (8) und dem Regelsystem für den wärmetransfer (6) eingefügt ist.
  10. Vorrichtung nach Anspruch 9, dadurch gekennzeichnet, daß sie einen Rückhaltebehälter (2) für das Target (1) umfaßt, dessen Boden (3) in einem wärmeleitfähigen Material ausgeführt ist und in den in Form von übereinander angeordneten Schichten das eventuelle Heizsystem (4), das Kühlsystem (5) und das Regelsystem (6) eingebettet sind.
  11. Vorrichtung nach Anspruch 10, dadurch gekennzeichnet, daß das eventuelle Heizsystem (4) in der Nähe des Targets (1) angeordnet ist.
  12. Vorrichtung nach einem der Ansprüche 9 bis 11, dadurch gekennzeichnet, daß das System zur Regelung des Wärmetransfers (6) einen Kreislauf aus flüssigem Metall umfaßt, insbesondere aus Gallium, und Mittel vorgesehen sind, um das Metall aus diesem Kreislauf zu entfernen, wenn eine Zufuhr von Wärme erforderlich ist, und um Metall in den Kreislauf einzuspeisen, wenn Wärme vom Target (1) abgeführt werden muß.
  13. Vorrichtung nach einem der Ansprüche 9 bis 12, dadurch gekennzeichnet,
    daß sie zwei Meßfühler (S1 und S2) zum Messen der Höhe der flüssigen Schicht (8) des Targets (1) umfaßt,
    der eine (S1) für die maximale Höhe und der andere (S2) für die minimale Höhe,
    wobei jeder der Meßfühler vorzugsweise über den Vergleich der gemessenen Spannung mit der Spannung des Targets (1) arbeitet.
  14. Vorrichtung nach einem der Ansprüche 9 bis 13, dadurch gekennzeichnet, daß sie einen Mechanismus (12) zur Beschickung der Oberflächenschicht (8) des Targets (1) mit dem zu zerstäubenden Metall umfaßt, sobald die Dicke der letzteren unterhalb eines vorher festgelegten Grenzwertes fällt.
  15. Vorrichtung nach einem der Ansprüche 13 und 14, dadurch gekennzeichnet,
    daß sie einen Meßfühler (S3) zur Bestimmung und zur Kontrolle der Temperatur (Tm) der Oberflächenschicht (8) des Targets (1) umfaßt,
    wobei dieser Meßfühler (S3) es ermöglicht, auf das System zur Regelung des Wärmetransfers (6) einzuwirken und die Oberflächenschicht (8) des Targets (1) auf eine Temperatur (Tm) oberhalb ihrer Schmelztemperatur zu bringen während sie mit dem zu schmelzenden Metall beschickt wird.
  16. Vorrichtung nach einem der Ansprüche 9 bis 15, dadurch gekennzeichnet, daß das Substrat (17) in Form eines Endlosstreifens vorliegt, der sich durch mindestens eine Kammer (15, 16), in welcher ein Target (1) angeordnet ist, bewegt.
  17. Vorrichtung nach Anspruch 16, dadurch gekennzeichnet, daß sie zwei aufeinander folgende Kammern (15) und (16) umfaßt, um die beiden Seiten des Streifens (17) zu beschichten,
    wobei in einer der Kammern (15) das Target (1) zu einer Seite des Streifens (17) und in der anderen Kammer (16) zu seiner entgegengesetzten Seite hin angeordnet ist.
EP95870065A 1994-06-02 1995-06-02 Verfahren und Vorrichtung zur Beschichtung eines Substrats mittels Kathodenzerstäubung Expired - Lifetime EP0685571B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
BE9400552 1994-06-02
BE9400552A BE1008303A3 (fr) 1994-06-02 1994-06-02 Procede et dispositif pour la formation d'un revetement sur un substrat par pulverisation cathodique.

Publications (2)

Publication Number Publication Date
EP0685571A1 EP0685571A1 (de) 1995-12-06
EP0685571B1 true EP0685571B1 (de) 1998-12-16

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EP95870065A Expired - Lifetime EP0685571B1 (de) 1994-06-02 1995-06-02 Verfahren und Vorrichtung zur Beschichtung eines Substrats mittels Kathodenzerstäubung

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EP (1) EP0685571B1 (de)
AT (1) ATE174637T1 (de)
BE (1) BE1008303A3 (de)
DE (1) DE69506618T2 (de)
DK (1) DK0685571T3 (de)
ES (1) ES2128028T3 (de)
GR (1) GR3029503T3 (de)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6432281B2 (en) * 1995-12-20 2002-08-13 Recherche Et Developpement Due Groupe Cockerill Sambre Process for formation of a coating on a substrate
BE1009838A3 (fr) * 1995-12-20 1997-10-07 Cockerill Rech & Dev Procede et dispositif pour la formation d'un revetement sur un substrat.
BE1010797A3 (fr) * 1996-12-10 1999-02-02 Cockerill Rech & Dev Procede et dispositif pour la formation d'un revetement sur un substrat, par pulverisation cathodique.
EP1182272A1 (de) 2000-08-23 2002-02-27 Cold Plasma Applications C.P.A. Verfahren und Vorrichtung zur kontinuierlichen Kaltplasma-Abscheidung von Metallschichten
JP2022505534A (ja) * 2018-10-24 2022-01-14 エヴァテック・アーゲー 液体スパッタターゲット

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2528108B2 (de) * 1975-06-24 1977-11-03 Siemens AG, 1000 Berlin und 8000 München Verfahren zum aufbringen von elektrisch leitenden schichten auf eine unterlage
JPH0192384A (ja) * 1987-10-02 1989-04-11 Hitachi Ltd プラズマ処理装置
JPH0219466A (ja) * 1988-07-07 1990-01-23 Matsushita Electric Ind Co Ltd 繊維・フィルム連続蒸着装置

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Publication number Publication date
ATE174637T1 (de) 1999-01-15
ES2128028T3 (es) 1999-05-01
BE1008303A3 (fr) 1996-04-02
GR3029503T3 (en) 1999-05-28
DK0685571T3 (da) 1999-08-23
EP0685571A1 (de) 1995-12-06
DE69506618T2 (de) 1999-07-08
DE69506618D1 (de) 1999-01-28

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